CN110251433B - Nymphaea hybrid extract, preparation method thereof, nymphaea hybrid water containing same and lotus moisturizing Shu Minshui - Google Patents

Nymphaea hybrid extract, preparation method thereof, nymphaea hybrid water containing same and lotus moisturizing Shu Minshui Download PDF

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CN110251433B
CN110251433B CN201910626527.8A CN201910626527A CN110251433B CN 110251433 B CN110251433 B CN 110251433B CN 201910626527 A CN201910626527 A CN 201910626527A CN 110251433 B CN110251433 B CN 110251433B
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nymphaea hybrid
water
extract
nymphaea
lotus
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CN110251433A (en
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雷登凤
吴新星
高合意
曾飒
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Guangzhou Ridgepole Biological Technology Co ltd
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/33Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/34Alcohols
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/73Polysaccharides
    • A61K8/735Mucopolysaccharides, e.g. hyaluronic acid; Derivatives thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/92Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof
    • A61K8/922Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof of vegetable origin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/96Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
    • A61K8/97Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
    • A61K8/9783Angiosperms [Magnoliophyta]
    • A61K8/9789Magnoliopsida [dicotyledons]
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin
    • A61Q19/005Preparations for sensitive skin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin
    • A61Q19/08Anti-ageing preparations
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/59Mixtures
    • A61K2800/592Mixtures of compounds complementing their respective functions
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/80Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
    • A61K2800/805Corresponding aspects not provided for by any of codes A61K2800/81 - A61K2800/95

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Abstract

The invention discloses a nymphaea hybrid extract, a preparation method thereof, nymphaea hybrid water containing the same and lotus moisturizing Shu Minshui. This extract of nymphaea hybrid contains amino acids and mineral elements and no pigments. The nymphaea hybrid extract is obtained by firstly carrying out hot extraction on nymphaea hybrid in water, and then carrying out decoloration and membrane treatment. The obtained nymphaea hybrid extract has good antioxidant effect, safety and stability. Simple operation and low cost. In the invention, the nymphaea hybrid water and lotus moisturizing Shu Minshui are obtained based on the nymphaea hybrid extract. The obtained nymphaea hybrid water has instant and long-acting moisturizing effect and remarkably improved silky skin feeling. The obtained lotus moisturizing Shu Minshui is mild and non-irritant to skin, and has good moisturizing effect.

Description

Nymphaea hybrid extract, preparation method thereof, nymphaea hybrid water containing same and lotus moisturizing Shu Minshui
Technical Field
The invention belongs to the technical field of cosmetics, and particularly relates to a nymphaea hybrid extract, a preparation method thereof, nymphaea hybrid water containing the same and lotus moisturizing Shu Minshui.
Background
In recent years, inflammatory diseases of the skin caused by various factors such as environmental pollution, pressure of life, and use of cosmetics have been increasing, and the incidence of skin irritation and allergic phenomena has been increasing, and there are increasing groups of people who feel sensitive skin by themselves. Therefore, the research and development of cosmetics with anti-inflammatory and allergy-relieving effects aiming at people with inflammatory skin are more and more concerned and favored by industries and consumers. The generation of sensitive skin is often related to skin barrier dysfunction, and moisturizing is the basis of barrier repair, so that the water retention capacity of the skin is improved, and the repair of the skin barrier can be effectively promoted; the soothing component can reduce anaphylactic reaction of sensitive skin and reduce over-strong reaction of nerves to external stimulation, thereby avoiding the generation of immune inflammation.
The nymphaea hybrid is rich in natural active ingredients such as polyphenol, flavone, polysaccharide, protein, trace elements and the like, and has remarkable whitening, moisturizing, antioxidant and other effects. At present, aiming at the development and application of the nymphaea hybrid, substances such as polyphenol, flavone and the like in the nymphaea hybrid are mostly extracted by ethanol and are applied to the development of cosmetics as functional components for whitening, resisting aging and the like. CN108553378A is prepared by ethanol ultrasonic extraction and reduced pressure rotary steaming to obtain a nymphaea hybrid extract. CN109303734A provides a nymphaea hybrid extract, which is obtained by enzymolysis, ethanol hot reflux extraction, vacuum concentration and vacuum freeze-drying. Both of these extraction processes introduce agents (e.g., ethanol) that may be irritating to the skin, thereby possibly causing skin irritation. Meanwhile, the two methods for preparing the nymphaea hybrid extract are relatively complex, and the cost is increased due to the use of reagents and equipment with higher price. In addition, the development and utilization of amino acids and mineral elements in the nymphaea hybrid are not disclosed.
Therefore, the soothing and moisturizing product which fully utilizes amino acids and mineral elements in the nymphaea hybrid is developed, and the process has the advantages of simple operation and low cost and has great market prospect.
Disclosure of Invention
In order to solve the problems, the invention provides a nymphaea hybrid extract, a preparation method thereof, nymphaea hybrid water containing the same and lotus moisturizing Shu Minshui. The nymphaea hybrid extract contains amino acids and mineral elements and does not contain pigments and other unstable components, and is fully developed and utilized through fine extraction of the nymphaea hybrid. Because no other chemical agents are contacted or introduced in the production process, potential skin allergy reaction can not be caused. And the nymphaea hybrid extract has good stability due to decolorization and membrane filtration treatment. The whole production operation is simple, and the cost of the reagent and the instrument is low. The nymphaea hybrid water obtained by compounding the nymphaea hybrid extract and hyaluronic acid in a reasonable proportion has the effects of relieving and moisturizing. The lotus moisturizing Shu Minshui prepared from the water of the nymphaea hybrid is mild and non-irritant to skin, and has a good moisturizing effect.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the present invention provides a nymphaea hybrid extract comprising amino acids and mineral elements and no pigments and other labile components.
In the prior art, substances in the nymphaea hybrid are generally extracted by using organic reagents such as ethanol and the like, amino acids and mineral elements contained in the nymphaea hybrid cannot be extracted, and the nymphaea hybrid extract containing the amino acids and the mineral elements has good antioxidant effect.
In a second aspect, the present invention provides a method for preparing a nymphaea hybrid extract according to the first aspect, comprising the steps of:
(1) Carrying out hot extraction on nymphaea hybrid in water to obtain an extracting solution;
(2) Carrying out decoloring treatment to obtain a decoloring extracting solution;
(3) Centrifuging and filtering to obtain nymphaea hybrid extract.
The amino acid and mineral elements in the nymphaea hybrid are extracted by water, so that the potential skin allergy-causing reaction caused by other agents (such as ethanol) is overcome. In addition, other chemical reagents are not introduced in the whole preparation process, and the safety of the nymphaea hybrid extract is also ensured.
Because of the instability of pigments and macromolecular substances, the nymphaea hybrid extract in the prior art can not be completely and stably stored, but the pigment and other unstable substances are effectively removed and the stability of the nymphaea hybrid extract is improved on the premise of ensuring the functional components through decolorization and membrane filtration treatment.
The whole preparation process has simple steps, does not need expensive reagents and instruments, has low cost and is suitable for large-scale production.
In the invention, the ratio of the nymphaea hybrid to water is 1.
Preferably, the water is deionized water.
Preferably, the temperature of the thermal extraction is 80-100 ℃, for example, 80 ℃, 85 ℃, 87 ℃, 90 ℃, 93 ℃, 96 ℃ or 100 ℃.
Preferably, the heat extraction time is 0.5 to 3h, for example, 0.5h, 1h, 1.6h, 1.9h, 2.2h, 2.5h, 2.7h or 3h.
Preferably, the step (1) further comprises filtering and cooling. Specifically, after the hot extraction, the supernatant is filtered and then cooled.
In the invention, activated carbon is adopted for the decolorization treatment in the step (2).
Preferably, the activated carbon is used in an amount of 0.03 to 0.1%, for example, 0.03%, 0.05%, 0.06%, 0.07%, 0.09%, or 0.1% based on 100% by mass of the extract solution.
Preferably, the time for the decoloring treatment with the activated carbon is 0.5 to 2 hours, and for example, may be 0.5 hour, 0.7 hour, 0.8 hour, 1 hour, 1.3 hours, 1.5 hours, 1.8 hours, or 2 hours.
The invention removes the pigment and other unstable substances in the nymphaea hybrid extract by controlling the temperature of the thermal extraction, the concentration of the active carbon used for the decoloration treatment and the decoloration time which are matched with each other.
In the invention, the filtration treatment in the step (3) adopts membrane filtration.
Preferably, the membrane has a pore size of 0.001 to 0.1. Mu.m, and may be, for example, 0.001. Mu.m, 0.005. Mu.m, 0.01. Mu.m, 0.02. Mu.m, 0.04. Mu.m, 0.05. Mu.m, 0.07. Mu.m, 0.08. Mu.m, 0.09. Mu.m, or 0.1. Mu.m.
The preparation method of the nymphaea hybrid extract comprises the following steps:
(1) Extracting herba seu radix Helianthi with water at 80-100 deg.C, filtering, and cooling;
(2) Decoloring by using activated carbon;
(3) And (4) performing centrifugation and membrane filtration treatment to obtain the nymphaea hybrid extract.
In a third aspect, the present invention provides a nymphaea hybrid water, comprising an nymphaea hybrid extract according to the first aspect.
Preferably, the nymphaea hybrid water further comprises hyaluronic acid.
Preferably, the hyaluronic acid is added in an amount of 0.05-0.5%, for example, 0.05%, 0.1%, 0.15%, 0.2%, 0.23%, 0.3%, 0.36%, 0.4%, 0.45%, or 0.5% based on 100% by mass of the water.
The preparation method of the water containing the perfume lotus flower comprises the following steps:
adding hyaluronic acid into the nymphaea hybrid extract, and then carrying out thermal degradation treatment to obtain the nymphaea hybrid water.
The nymphaea hybrid extract is compounded with hyaluronic acid, so that the nymphaea hybrid water has the effects of relieving and moisturizing and is available for people with sensitive skin. The method comprises the following steps of carrying out thermal degradation treatment to cut macromolecular substances into micromolecular substances with different molecular weights, and endowing the lotus water for perfume with instant moisturizing and deep long-acting moisturizing effects by controlling reasonable proportion combination and a thermal degradation process; the small molecular substance is easier to permeate the structure of the horny layer, so that the biological activity of the flower water can be exerted to the maximum extent; meanwhile, the skin feeling of the perfume lotus flower water is greatly improved through the combination and matching treatment.
Preferably, the equipment for thermal degradation treatment is a sterilizer, and further preferably a horizontal sterilizer.
The time for the thermal degradation treatment is preferably 10min to 4 hours, and may be, for example, 10min, 15min, 30min, 40min, 55min, 1.5 hours, 2 hours, 3 hours, or 4 hours, and more preferably 15min to 45min.
Preferably, the thermal degradation treatment temperature is 90-130 ℃, for example, can be 90 ℃,95 ℃, 100 ℃, 105 ℃, 118 ℃, 120 ℃, 125 ℃ or 130 ℃, more preferably 100-121 ℃.
Preferably, the step of the preparation method further comprises adding a thickener.
Preferably, the thickener is hydroxyethyl cellulose.
Preferably, the amount of hydroxyethyl cellulose is 0-0.1%, for example, 0%, 0.02%, 0.04%, 0.05%, 0.07%, 0.08% or 0.1% by mass of the nymphaea hybrid extract, based on 100% by mass of the nymphaea hybrid extract.
In a fourth aspect, the present invention provides the use of a nymphaea hybrid extract according to the first aspect or a nymphaea hybrid water according to the third aspect for the preparation of a cosmetic.
In a fifth aspect, the invention provides a lotus moisturizing Shu Minshui comprising a nymphaea hybrid extract according to the first aspect or a nymphaea hybrid water according to the third aspect.
Preferably, the lotus moisturizing and allergy-relieving water also comprises an anti-allergy composition.
The anti-allergy composition is disclosed in patent CN108175717A, and comprises ginger essential oil and bisabolol.
Preferably, the anti-allergy composition is used in an amount of 0.1-2%, for example, 0.1%, 0.2%, 0.5%, 0.7%, 1%, 1.3%, 1.5%, 1.8% or 2%, based on 100% of the lotus moisturizing Shu Minshui.
The obtained lotus moisturizing Shu Minshui is mild and non-irritating to skin, and has effects of activating cells, moisturizing and relieving.
Compared with the prior art, the invention has the following beneficial effects:
(1) The nymphaea hybrid extract fully develops and utilizes amino acids and mineral elements in the nymphaea hybrid, does not contain pigments and other unstable components, and has good antioxidant effect.
(2) No other chemical reagent is contacted or introduced in the production process, so that the safety of the nymphaea hybrid extract is ensured.
(3) Decolorizing and membrane filtering to remove unstable pigment and macromolecular substances while ensuring efficacy, so that the extract of herba Hylotelephii Erythrosticti has good stability (at 55 deg.C, after 14 days).
(4) Simple operation, low cost and suitability for large-scale production.
(5) The nymphaea hybrid extract is compounded with hyaluronic acid in a reasonable proportion, and the obtained nymphaea hybrid water has the effects of relieving and moisturizing. The preparation process adopts thermal degradation treatment, so that the lotus perfume water has the effects of instant and long-acting moisture preservation, and the silky skin feeling of the lotus perfume water is obviously improved.
(6) The lotus moisturizing Shu Minshui is mild and non-irritant to skin, and has a good moisturizing effect.
Detailed Description
The technical solution of the present invention is further explained by the following embodiments. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
Example 1
Taking dried nymphaea hybrid whole flowers, removing insect pests and mildewed parts, adding deionized water according to the material-liquid ratio of 1.
Example 2
Taking dried nymphaea hybrid whole flowers, removing insect pests and mildewed parts, adding deionized water according to the material-liquid ratio of 1.
Example 3
Taking dried nymphaea hybrid whole flowers, removing insect pests and mildewed parts, adding deionized water according to the material-liquid ratio of 1.
Comparative examples 1 to 2
The only difference from example 1 was that the thermal extraction temperature was 70 deg.C (comparative example 1) and 110 deg.C (comparative example 2).
Comparative examples 3 to 4
The only difference from example 1 was that the activated carbon concentration was 0.01wt% (comparative example 3), 0.2wt% (comparative example 4).
Comparative examples 5 to 6
The difference from example 1 is that the time for the decoloring treatment was 20min (comparative example 5) and 2.2h (comparative example 6).
Comparative examples 7 to 8
The difference from example 1 is that the pore size of the organic filter membrane is 0.0005 μm (comparative example 7) and 0.2 μm (comparative example 8).
Performance test 1
The nymphaea hybrid extracts provided in examples 1-3 and comparative examples 1-8 were subjected to a performance test as follows:
(1) And (3) testing the stability:
the samples obtained in examples 1 to 3 and comparative examples 1 to 8 were placed in an oven at 55 ℃ for 14 days for thermal stability evaluation: the absorbance (OD value) was measured at 450nm, and the color was observed. Wherein, A-is colorless and clear, B-is light yellow and clear, C-is yellow and clear, and D-is yellow and turbid.
(2) And (3) testing the oxidation resistance:
the antioxidant properties of the samples obtained in examples 1-3 and comparative examples 1-8 are illustrated by DPPH radical scavenging ratio. Accurately weigh 0.2500g of DPPH into a small beaker, dissolve with 95% methanol and transfer to a 1000mL volumetric flask, and hold the volume to obtain 250. Mu.g/mL DPPH stock solution, which is kept in refrigeration until use (ready for use). Accurately transferring the stock solution into a volumetric flask of 10mL to 50mL, and diluting the stock solution with 95% methanol to a constant volume to obtain a DPPH standard solution of 50 mu g/mL. Then prepare 100, 150, 200 mug/mL DPPH standard solution respectively. The DPPH scavenging ability was measured spectrophotometrically (517 nm). The positive control was 0.5% water soluble VE.
The DPPH free radical clearance (K) is calculated by the following method:
K=[1-(A 1 -A 2 )/A 0 ]×100%;
A 1 : 1mL of sample and 3mL of DPPH solution are uniformly mixed, and the light absorption value is measured at 517 after 20min;
A 2 : 1mL sample and 3mL 95% methanol solution are mixed evenly, and after 20min, the light absorption value is measured at 517;
A 0 : taking 1mL of deionized water, and then taking DPPHThe solution was 3mL, mixed well and absorbance was measured at 517 after 20 min.
(3) Hyaluronidase inhibition assay:
taking 0.1mL of CaCl 2 Incubating and culturing the solution (0.25 mmol/L) and 0.5mL hyaluronidase solution at 37 ℃ for 20min; adding 0.5mL of sample liquid, and carrying out heat preservation culture at 37 ℃ for 20min; adding 0.5mL sodium hyaluronate solution, keeping the temperature at 37 ℃ for 30min, and standing at normal temperature for 5min; adding 0.1mL of NaOH solution (0.4 mol/L) and 0.5mL of acetylacetone solution, heating in a boiling water bath for 15min, and immediately cooling for 5min; 1.0mL of an Ellisib reagent was added, and the mixture was diluted with 3.0mL of absolute ethanol and allowed to stand for 20min for color development. The absorbances of the samples obtained in application examples 1 to 5 and application comparative examples 1 to 5 were measured at 585nm, and then the hyaluronidase inhibition ratios were calculated, respectively. The positive control is 0.1% dipotassium glycyrrhizinate aqueous solution.
The calculation method of the hyaluronidase inhibition rate comprises the following steps:
hyaluronidase inhibition (%) = [ (C-D) - (A-B) ]/(C-D) × 100%;
a: OD value of (hyaluronidase + sample + sodium hyaluronate) test sample solution;
b: OD value of a blank sample (acetic acid buffer solution + sample + acetic acid buffer solution);
c: OD value of control solution (hyaluronidase + deionized water + sodium hyaluronate);
d: (acetate buffer + deionized water + acetate buffer) control blank OD value.
The test results are shown in table 1:
TABLE 1
Stability of Oxidation resistance (%) Hyaluronidase inhibition (%)
Example 1 A 73 85
Example 2 A 74 89
Example 3 A 71 87
Comparative example 1 A 63 76
Comparative example 2 B 69 79
Comparative example 3 C 73 85
Comparative example 4 A 57 63
Comparative example 5 C 71 88
Comparative example 6 A 61 54
Comparative example 7 A 32 21
Comparative example 8 D 72 89
As can be seen from Table 1, under the test condition of 55 ℃, within 14 days, the examples are always kept as colorless and clear liquid with lower and stable OD values, which shows that the nymphaea hybrid extract prepared by the process has good thermal stability and provides a basis for the stability of products for subsequent applications.
The skin barrier can effectively prevent the invasion of external harmful substances, and the damage of the skin barrier is one of the main reasons of sensitive muscles. Free radicals in a human body can attack cell membranes, proteins and even DNA, so that the aging and even death of cells are caused, and the inhibition of the free radicals can effectively relieve the degradation of cell structure functions caused by excessive free radicals generated by external stimulation, thereby maintaining the normal barrier function of the skin. As can be seen from table 1, the examples have a large scavenging capacity for free radicals, which indicates that the nymphaea hybrid extract has a good antioxidant capacity. Compared with comparative examples 1, 2, 3, 4, 6 and 7, the examples have stronger DPPH free radical scavenging capacity, which shows that the extraction process, the decolorization and purification process of activated carbon and the membrane filtration process have more obvious influence on the antioxidant effect of the nymphaea hybrid extract.
Hyaluronidase is a specific lyase of hyaluronic acid, and inhibition of hyaluronidase activity can ensure the content and normal function of hyaluronic acid. Research shows that hyaluronidase has strong correlation with inflammation and allergy, and many antiallergic drugs have strong effect of inhibiting the activity of hyaluronidase. As can be seen from Table 1, the examples have a strong inhibitory effect on hyaluronidase, which indicates that the nymphaea hybrid extract has a good allergy-relieving effect. Compared with comparative examples 1, 2, 3, 4, 6 and 7, the examples have stronger hyaluronidase inhibition effect, which shows that the extraction process, the decolorization and purification process of activated carbon and the membrane filtration process have more obvious influence on the allergy-relieving efficacy of the nymphaea hybrid extract.
By comparing example 1 with comparative examples 1 to 8, it can be seen that the obtained nymphaea hybrid extract has better stability when the hot extraction temperature is 80 to 100 ℃, the activated carbon concentration is 0.03 to 0.1% and the decoloring treatment time is 0.5 to 2 hours. When the hot extraction temperature is lower than 80 ℃, the microorganisms in the extracting solution cannot be completely removed; when the temperature is higher than 100 ℃, a large amount of pigment is extracted, and the extract is difficult to decolor. When the amount of the activated carbon is less than 0.03% or the time for the decoloring treatment is less than 0.5h, the pigment is not completely removed due to insufficient decoloring treatment, thereby causing a decrease in stability. However, when the amount of activated carbon is more than 0.1% or the time for decoloring is more than 2 hours, amino acids and mineral elements in the nymphaea hybrid extract are also adsorbed, so that the antioxidant effect is reduced. When the pore diameter of the organic filter membrane is less than 0.001 mu m, most of active ingredients are filtered, so that the activity of the organic filter membrane is greatly reduced; when the pore diameter of the organic filter membrane is larger than 0.1 μm, many unstable macromolecular substances in the extracting solution are not filtered, so that precipitates can be separated out from the extracting solution.
Application example 1
Adding 0.05% hyaluronic acid and 0.01% hydroxyethyl cellulose into the nymphaea hybrid extract obtained in example 1, and treating in a horizontal sterilizer for 2h at 100 deg.C to obtain nymphaea hybrid water.
Application example 2
Adding 0.5% hyaluronic acid into the nymphaea hybrid extract obtained in example 1, and treating in a horizontal sterilizer at 130 deg.C for 10min to obtain nymphaea hybrid water.
Application example 3
0.05 percent of hyaluronic acid and 0.1 percent of hydroxyethyl cellulose are added into the nymphaea hybrid extract obtained in the example 1, and the mixture is treated in a horizontal sterilizer for 4 hours at the treatment temperature of 90 ℃ to obtain the nymphaea hybrid water.
Application example 4
Adding 0.05% hyaluronic acid and 0.01% hydroxyethyl cellulose into the nymphaea hybrid extract obtained in example 1, and treating for 15min in a horizontal sterilizer at 121 ℃ to obtain nymphaea hybrid water.
Application example 5
Adding 0.05% hyaluronic acid and 0.01% hydroxyethyl cellulose into the nymphaea hybrid extract obtained in example 1, and treating for 45min in a horizontal sterilizer at 100 deg.C to obtain nymphaea hybrid water.
Application comparative example 1
The only difference from application example 1 is that the nymphaea hybrid extract was replaced with deionized water.
Comparative application example 2
The difference from application example 1 is that in the present application comparative example, hyaluronic acid is not included, and the amount of the nymphaea hybrid extract is the sum of the added amounts of hyaluronic acid and the nymphaea hybrid extract in application example 1.
Comparative application example 3
The difference from application example 1 is that in the present comparative application example, only hyaluronic acid was included, and the added amount thereof was the sum of the added amounts of hyaluronic acid and the nymphaea hybrid extract in application example 1.
Application comparative example 4
The difference from application example 1 is that the treatment was carried out in a horizontal sterilizer for 5min at a treatment temperature of 140 ℃.
Comparative application example 5
The difference from application example 1 is that the treatment was carried out in a horizontal sterilizer for 5 hours at a treatment temperature of 80 ℃.
Performance test 2
The performance test is carried out on the water for perfume lotus flower provided by the application examples 1-5 and the application comparative examples 1-5, and the method comprises the following steps:
(1) Sensory evaluation:
subject 10, mean age 26.8 years. And (3) respectively smearing the samples obtained in the application examples 1-5 and the application comparative examples 1-5 on different parts of the back and the arm of each person, recording the use feeling, and grading different test indexes according to the standard. The scores of the 3 indexes (sticky feeling, absorption speed and water wetness) are tested, the score of each index is 0-3, and then the average score of the three indexes is calculated respectively. Higher scores indicate poorer skin feel. Wherein: sticky feeling (0: fresh and not sticky; 1: slightly sticky; 2: more sticky; 3: extremely sticky; speed of absorption (0: quick absorption; 1: light pat absorption; 2: hard absorption; 3: substantially non-absorption; degree of hydration (0: very moist; 1: comparatively moist; 2: drier; 3: very dry)
The test results are shown in table 2:
TABLE 2
Figure BDA0002127291750000121
Figure BDA0002127291750000131
From table 2, it can be seen that, in combination of 3 indexes, the application examples 4 and 5 have good skin feel due to the temperature of the thermal degradation treatment being in the range of 100 to 121 ℃ and the time being in the range of 15 to 45min, while the application comparative examples 4 to 5 have poor performance in terms of sticky feel, water-wet effect, and tight feel due to the possibility that the proportion of high molecular weight hyaluronic acid is low or high due to the temperature of the thermal degradation treatment being not in the range of 90 to 130 ℃ and the time being not in the range of 10min to 4 h.
(2) Barrier repair experiments:
20 subjects, washed their arms, marked 4X 4cm in the forearms of the left and right hands 2 A test area; in constant temperature and humidity experimentResting in room (temperature: 21 + -1 deg.C, relative humidity: 45 + -5%) for 5min, and testing the initial skin transdermal water loss value (TEWL) of the arm First stage ) (ii) a Then, the first skin barrier of the subject is destroyed by a tape tearing method, and then the arm skin percutaneous water loss value (TEWL) of the subject is rapidly tested 0 ) (ii) a Then, the samples obtained in application examples 1 to 5 and application comparative examples 1 to 5 (used amount: 2.0. + -. 0.1. Mu.L/cm) 2 ) Smearing on the damaged area of the barrier, and testing TEWL at 1h, 2h, 4h and 6h 1 、TEWL 2 、TEWL 4 、TEWL 6
The test results are shown in table 3:
TABLE 3
Figure BDA0002127291750000132
Figure BDA0002127291750000141
The rate of repair of the skin barrier by the smeared samples over time was calculated from the TEWL values of table 3 by:
barrier repair rate (%) = (TEWL) 0 -TEWL Time )/(TEWL 0 -TEWL Beginning of the design ) Wherein TEWL Time Taking TEWL 1 、TEWL 2 、TEWL 4 、TEWL 6
From table 3 we can calculate that the skin barrier repair rate of the application examples over time is much greater than that of the comparative application examples, wherein the skin barrier repair rate of the application examples 1-5 is between 55-70% and that of the comparative application examples 1-5 is between 30-45% after 6 hours of sample application; it can also be seen from the absolute value of the transdermal water loss that the absolute value of the transdermal water loss after the sample is smeared is much larger in the application examples 1 to 5 than in the application comparative examples 1 to 5. Therefore, the content of hyaluronic acid and the temperature and time for thermal degradation have great influence on the barrier repair effect of the perfume lotus flower water.
Application example 6
5% of glycerin, 4% of butanediol, 0.05% of EDTA-Na, 1% of panthenol, 2% of avenanthramides, 0.2% of an anti-allergy composition and the nymphaea hybrid water obtained in application example 1 were mixed to 100% to obtain a lotus moisturizing Shu Minshui.
Performance test 3
Safety and efficacy evaluations were performed on lotus moisturizing Shu Minshui provided in application example 6, the method was as follows:
(1) Patch testing
And (5) evaluating the safety by adopting a patch test. Subject 36 (male 9, female 27) who met the volunteer enrollment criteria; spot tester (Beijing science popularization Instrument factory), about 0.020-0.025mL of the sample obtained in application example 6 was applied to a spot tester cell by a closed spot test method, a special adhesive tape was applied to the back of the subject, the spot tester was removed after 24 hours, and if the remaining sample was wiped off with a moist paper towel, the results were recorded at 0.5 hour, 24 hours, and 48 hours, respectively, according to the skin reaction grading standard in the technical Specification for cosmetics safety (2015). Skin response grading criteria (see technical Specification for cosmetic safety (2015)).
The test results were as follows:
in the patch test, 36 subjects did not show any reaction and no adverse reaction, such as erythema, burning sensation or pruritus, according to the data of 30 minutes, 24 hours and 48 hours. The enclosed patch test shows that the lotus moisturizing Shu Minshui prepared from the flower water has no irritation to skin.
(2) Moisture retention test
And (5) evaluating the efficacy by adopting a moisture retention test. 15 subjects, washed their arms, marked 4X 4cm in the forearms of the left and right hands 2 A test area; resting in a constant temperature and humidity laboratory (temperature: 21 +/-1 ℃, relative humidity: 45 +/-5%) for 5 minutes, and testing the initial moisture content of the horny layer of the skin (MMV value) and the transdermal water loss value of the skin (TEWL value) of the arm of the subject; the sample obtained in application example 6 and a blank sample (used in an amount of 2.0. + -. 0.1. Mu.L/cm) 2 ) The test area is evenly coated, and then the MMV value and the TEWL value are tested at 1h, 2h, 4h and 6 h. The blank sample is the sample obtained in application example 6 without adding perfume lotus flower waterA composition is provided.
The results of the test for stratum corneum moisture content and skin transdermal water loss at each time point are shown in table 4:
TABLE 4
Figure BDA0002127291750000161
As can be seen from Table 4, after the lotus flower moisturizing liquid is applied for Shu Minshui h, the skin moisture content is still remarkably increased, and the effect of obviously reducing the loss of skin moisture is achieved, so that the lotus flower moisturizing and allergy relieving liquid has a good moisturizing effect.
The applicant states that the present invention is illustrated by the above examples to show the detailed method of the present invention, but the present invention is not limited to the above detailed method, that is, it does not mean that the present invention must rely on the above detailed method to be carried out. It should be understood by those skilled in the art that any modification of the present invention, equivalent substitutions of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.

Claims (10)

1. The preparation method of the water with the lotus flowers is characterized by comprising the following steps of:
mixing the nymphaea hybrid extract, hydroxyethyl cellulose and hyaluronic acid, and then carrying out thermal degradation treatment at the temperature of 100-121 ℃ for 15-45min to obtain nymphaea hybrid water;
the addition amount of the hyaluronic acid is 0.05-0.5% by taking the mass of the nymphaea hybrid water as 100%;
the nymphaea hybrid extract contains amino acids and mineral elements and does not contain pigments, and the preparation method of the nymphaea hybrid extract comprises the following steps:
(1) Carrying out thermal extraction on nymphaea hybrid in water to obtain an extracting solution, wherein the temperature of the thermal extraction is 80-100 ℃;
(2) Performing decolorization treatment for 0.5-2h by using active carbon to obtain decolorized extract, wherein the active carbon is used in an amount of 0.03-0.1% by mass of the extract as 100%;
(3) Performing centrifugation and membrane filtration treatment, wherein the pore diameter of the membrane is 0.001-0.1 μm to obtain the nymphaea hybrid extract.
2. The method for preparing the water of nymphaea hybrid according to claim 1, wherein the equipment for the thermal degradation treatment is a horizontal sterilizer.
3. The method for preparing nymphaea hybrid water according to claim 1, wherein the amount of the hydroxyethyl cellulose is 0-0.1% by mass of the nymphaea hybrid extract as 100%.
4. The preparation method of the nymphaea hybrid water according to claim 1, wherein the ratio of the nymphaea hybrid extract to water in the step (1) is 1.
5. The method for preparing nymphaea hybrid water according to claim 1, wherein the heat extraction time in the step (1) is 0.5 to 3 hours.
6. The method for preparing nymphaea hybrid water according to claim 1, wherein the step (1) further comprises filtering and cooling.
7. Use of the nymphaea hybrid water prepared by the method for preparing the nymphaea hybrid water according to any one of claims 1 to 6 in the preparation of cosmetics.
8. An lotus moisturizing Shu Minshui, wherein the lotus moisturizing and allergy relieving water comprises the nymphaea hybrid water prepared by the method for preparing the nymphaea hybrid water according to any one of claims 1 to 6.
9. The lotus moisturizing Shu Minshui as in claim 8, wherein the lotus moisturizing and allergy relieving water further comprises an anti-allergy composition.
10. The lotus moisturizing Shu Minshui as in claim 9, wherein the amount of the anti-allergy composition is 0.1-2% by mass of the lotus moisturizing and allergy-relieving water of 100%.
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